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Mescaline HCl -> mesc (bi)tartrate recrystallization Options
 
1008
#1 Posted : 4/30/2009 8:45:16 PM
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SWIM has a bit of dirty brown mescaline HCL and wanted to purify it. Since the tartrate salt (and presumably the bitartrate salt) isn't very soluble in room temperature/cold water, he thought he'd just try recrystallizing as follows: Dissolve MescHCl in small volume of hot water, dissolve Na2tartrate or NaHtartrate in hot water, mix, then slowly cool and collect crystals.

The bitartrate should be significantly more massive/mole, which is nice for some reasons, but the driving factor would be the solubility in cold water- how much water can be used before losing too much goodies.

It would be very useful to know the solubilities before attempting this, so if anyone knows (even roughly), SWIM would love to know.

SWIM will make sure to get the results back to you guys, success or failure. Smile
 

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69ron
#2 Posted : 4/30/2009 10:11:08 PM

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SWIM tried making mescaline tartrate and had a hard time getting it to crystallize and gave up on it.

The best way to purify it and get white odorless mescaline HCl is to wash it with acetone 2-4 times and then with 99% IPA 1-3 times. You'll end up with 99% purity. It will be white, and completely odorless.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
1008
#3 Posted : 4/30/2009 10:16:46 PM
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Hmm...

From what little information was out there, it seemed like it should have been easy. Did you try crystallizing the bitartrate salt too?

How much mescaline is lost with the acetone/IPA washes and what what is the volume of solvent/gram impure mescaline that you used per "wash"?

Thanks

ETA: What about the fumarate salt? I seem to remember you (69ron) saying you were going to check it out, but didn't see the results of that.
 
69ron
#4 Posted : 5/1/2009 7:06:24 PM

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You’d wash a gram of mescaline in about 20-40 ml of acetone. You mix it thoroiughly and smash it while mixing it to make sure most of the brown impurities dissolve in the acetone. Then you let it sit in the refrigerator until all the mescaline HCl settles down. Then you simply decant the acetone. You repeat this about 2-3 times or until the mescaline doesn’t seem to be getting any lighter in color. After than you do the same with 99% IPA. It takes maybe 1-3 IPA washes. It MUST BE 99% IPA, no other alcohol will substitute. Mescaline HCl is very slitghtly soluble in acetone, so there will be a tiny bit of loss but it’s maybe 1-3% or so. Mescaline HCl is completely insoluble in 99% IPA, so there should be no loss from that step.

SWIM could NOT get the bitartrate salt to crystallize at all. He tried freeze precipitation, letting it evap, etc., nothing worked. Maybe there’s something he did wrong. It’s possible. SWIM also tried making mescaline citrate and had the exact same problems!

SWIM tried making mescaline fumarate, but couldn’t get it out of the d-limonene! It’s apparently soluble in d-limonene, so he gave up on that for now. He’ll revisit that.

SWIM's work with the bitartrate, the citrate, and the fumarate were done a long time ago and SWIM's cactus may have just been of extremely poor quality and that might be why he had such bad results.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
1008
#5 Posted : 5/1/2009 10:41:30 PM
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I'm a bit unclear on what exactly did and did not work. Let me attempt to summarize SWIY's experiments:
1) mescaline tartrate would not crystalize (did SWIY do this one?)
2) mescaline bitartrate would not crystalize
3) mescaline fumarate is soluble in d-limonene so crystallization was not attempted
4) mescaline citrate would not crystallize (though others report success)

These tests (except for one?) happened a while back and it is possible that there just wasn't enough mescaline there to crystallize.

Does that sound like a fair summary?

I'd like to know how likely it is that there just wasn't any mescaline in there and that we could go back to our prior (highish) probabilities that crystallization would be easy. I know SWIY had a bunch of trouble with mescaline extractions in the past (at least partly due to bunk cactus, and part due to washing the xylene with water), so if I'm understanding right, it seems like lack of mescaline is likely the reason it didn't crystallize, especially given that there is a report of mescaline tartrate crystallizing well, and several of citrate crystallizing.

If you think there's a decent chance recrystallization would work, SWIM would still like to give it a try for experimentation's sake (he can always redo a small scale A/B if it all fails). If not, SWIM will try acetone washes and then IPA washes. The only IPA SWIM could find locally was 70% so he salted it out and will dehydrate further with MgSO4- this should be good enough, right?

Thanks

 
69ron
#6 Posted : 5/1/2009 10:56:41 PM

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1008 wrote:
I'm a bit unclear on what exactly did and did not work. Let me attempt to summarize SWIY's experiments:
1) mescaline tartrate would not crystalize (did SWIY do this one?)
2) mescaline bitartrate would not crystalize
3) mescaline fumarate is soluble in d-limonene so crystallization was not attempted
4) mescaline citrate would not crystallize (though others report success)

These tests (except for one?) happened a while back and it is possible that there just wasn't enough mescaline there to crystallize.

Does that sound like a fair summary?


Exactly, so don't be too surprised if you have success even though SWIM didn't.

1008 wrote:
I'd like to know how likely it is that there just wasn't any mescaline in there and that we could go back to our prior (highish) probabilities that crystallization would be easy. I know SWIY had a bunch of trouble with mescaline extractions in the past (at least partly due to bunk cactus, and part due to washing the xylene with water), so if I'm understanding right, it seems like lack of mescaline is likely the reason it didn't crystallize, especially given that there is a report of mescaline tartrate crystallizing well, and several of citrate crystallizing.

If you think there's a decent chance recrystallization would work, SWIM would still like to give it a try for experimentation's sake (he can always redo a small scale A/B if it all fails). If not, SWIM will try acetone washes and then IPA washes. The only IPA SWIM could find locally was 70% so he salted it out and will dehydrate further with MgSO4- this should be good enough, right?

Thanks


No...you absolutely need 99% IPA for the final wash. No other substitute will work. If you can’t get 99% IPA, you can still clean up the mescaline HCl considerably with just the acetone washes. You can easily go from 75% pure dark brown mescaline HCl to about 95% pure light tan mescaline HCl with just acetone washes, but that final 5% is very stinky and only a 99% IPA wash can get it out without washing away the mescaline HCl. I don’t know what stores you have in your area but Safeway usually carries 99% IPA.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
1008
#7 Posted : 5/1/2009 11:06:19 PM
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Quote:

Exactly, so don't be too surprised if you have success even though SWIM didn't


In that case, SWIM will give it a try.

Quote:
No...you absolutely need 99% IPA for the final wash. No other substitute will work


Hmm.. I had a hard time finding reliable numbers for salted out IPA, but those that I did find said it was 99%. Is it that the 1% water is necessary (and this makes it too dry - 100% IPA won't work) or that salting and adding MgSO4 cant get close enough to anhydrous? There are other stores in SWIMs are that he hasn't checked, so if the crystallization thing doesn't work out, he'll look harder.

Thanks
 
970Codfert
#8 Posted : 5/1/2009 11:13:08 PM

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What is IPA?
All posts are fictional.
 
1008
#9 Posted : 5/2/2009 12:14:37 AM
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Quote:

What is IPA?


Isopropyl alcohol
 
69ron
#10 Posted : 5/2/2009 1:08:57 AM

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1008 wrote:
Quote:

Exactly, so don't be too surprised if you have success even though SWIM didn't


In that case, SWIM will give it a try.


Let me know how it works out.

1008 wrote:
Quote:
No...you absolutely need 99% IPA for the final wash. No other substitute will work


Hmm.. I had a hard time finding reliable numbers for salted out IPA, but those that I did find said it was 99%. Is it that the 1% water is necessary (and this makes it too dry - 100% IPA won't work) or that salting and adding MgSO4 cant get close enough to anhydrous? There are other stores in SWIMs are that he hasn't checked, so if the crystallization thing doesn't work out, he'll look harder.

Thanks


You want as little water as possible present in the IPA. 99% is the minimum you should use. 99.9% is not worth the extra price. 99% is plenty good enough for this purpose.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
1008
#11 Posted : 5/23/2009 9:31:31 PM
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SWIM told me that he finally got around to trying this.

Here is what he told me
Quote:
I weighed out 420mg of *dark* brown mescaline hydrochloride, and then weighed out 1000mg of tartaric acid and 250mg of NaOH (should produce a slight excess of sodium bitartrate even if the mescaline was pure). The acid and base were added to 2floz of hot water and then the mescaline was dissolved. This was filtered, and quite a bit of dark gunk came out.

The solution was then put in the freezer, but nothing crystallized out before it started to freeze. The solution was then poured in a glass baking dish and put in the oven at low heat to evaporate off some of the water. The oven was turned off after maybe an hour, but it wasn't checked until the next morning.

There are pretty crystals in the baking dish. There is still over half of a fluid ounce of liquid left over. I'm not sure if the crystals are sodium bitartrate or mescaline bitartrate, as the solubility of sodium bitartrate is low enough for it to have started crystallizing. I still have to separate the crystals from the solvent (scrape up and rinse with ice water?) and test the melting point.

If the mass is greater than it could be with just sodium bitartrate and the melting point != 253C (probably lower), then it's probably mescaline. I could also try crystallizing sodium bitartrate on its own to see if the crystals look similar or not. Of course, the final test is bioassay, but that isn't going to be for a while.

Any ideas?


SWIM told me he'd report back with more details as the experiment progresses.
 
Jorkest
#12 Posted : 5/23/2009 9:39:29 PM

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SWIM is trying to salt out mescaline fumarate..and didnt see this post...SWIM also found that it stayed in the d-limonene..but then he just let it sit for a few days..and what happened is that there are crystals floating between the layer of d-limonene and FASW(fumaric acid saturated water)...now hes just got to get it out...hes been thinking that he might be able to suck out the d-limonene as best as he can...or maybe the water first...the crystals should be on the bottom and he may be able to pour off the d-limonene..

ill get back to you after he tries it out
it's a sound
 
69ron
#13 Posted : 5/23/2009 11:32:20 PM

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SWIM tried that, but didn't let it sit that long. I hope those are actually mescaline and not fumaric acid crystals. When SWIM did it using FASA, fumaric acid precipitated out and the mescaline stayed in the d-limoneneSad
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
narmz
#14 Posted : 5/24/2009 1:10:39 AM

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After SWIM evapped the acetone used to clean up the product, the results had the consistency of tar. After evapping the iso, the results were light tan crystals very similar to the mesc hcl. SWIM is wondering if this is what others have experienced, and also, if it is possible that the product from the iso evap was actually unsettled mesc hcl, as SWIM did not use the fridge to settle the particles, and just waited until it looked like particles were no longer moving about in the iso.
Everything I post is made up fiction. SWIM represents a character who is not based in or on reality.
 
narmz
#15 Posted : 5/24/2009 4:21:05 AM

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So SWIM learned a couple things. The first is how important it is to break up the pieces in your acetone/iso clean-up, and the second is patience. SWIM decided to take all of his evaps from iso, and his finished product, and clean them up in iso one more time. He left it sitting in the fridge for a few hours, and has found that a layer of pure white powder has formed atop, so SWIM really was leaving some very pure mescaline in suspension by not allowing it enough time to separate. The layer that the white powder sits atop is a light tan layer, which obviously has not been broken into small enough pieces.
Everything I post is made up fiction. SWIM represents a character who is not based in or on reality.
 
1008
#16 Posted : 5/24/2009 5:54:32 AM
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SWIM told me he did some more work on it. Here's what he said:

Quote:
I poured it all in a coffee filter and let the water drip through. I then rinsed it a couple times with ice water.

I dried the liquid portion in the glass baking dish in the oven, and let the filter paper dry in the air. I ended up with these beautiful gold/beige looking crystals. The catch is that there's only 105mg of them =\. Theres 1.05g of the other crap that made it through the filter (which isn't pretty at all).

Assuming this is mescaline bitartrate, it is only 1/3 as potent as mescaline HCl and I only recovered ~10% of my original sample. Either it was *extremely* impure or the rest must be in the gunky crystalline stuff.

Another possibility (seems more likely) is that mescaline bitartrate is fairly soluble, but mescaline tartrate is not, and that my careless weighing was 15mg of NaOH too much, and therefore there was some tartrate anions in solution. Then mescaline tartrate crystallized out, but the rest of the mescaline was trapped as something that wouldn't crystallize.

The report here talks about "olive" colored "mescaline tartrate". "Olive" sounds like it could be describing the same color, and his crystals clearly were not very soluble so I think we're talking about the same substance. He seemed to use an excess of tartaric acid, so I would expect him to end up with the tartrate as opposed to the bitartrate.

This all seems to point in the direction of "mescaline bitartrate doesn't crystallize well, but mescaline tartrate does".

If all goes well, it looks like this could be a method for easy extraction (no AB bs). Just boil down to small volume, add excess tartaric acid and crystallize out. The crystals came out very pretty and pure looking even though the mescaline I started with was not very pure, so hopefully even without the nonpolar step a decent purity can be obtained (and a simple recrystallization should get more pure).

Tomorrow I will add more NaOH to convert the bitartrates to tartrates and see what happens. Wish me luck!



Does any of that make sense or is he crazy?
 
1008
#17 Posted : 5/26/2009 8:11:14 PM
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SWIM added NaOH up to ph = 7 and tried crystallizing more out. It didn't work- it just dies out into semi-crytalline gunk.

Any thoughts?
 
burnt
#18 Posted : 5/26/2009 8:27:29 PM

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SWIM would just say fuck it and just clean the mescaline HCl with anhydrous acetone. It works perfectly.

SWIM doesn't see need for IPA. Ron how do you know the mescaline gets more pure when one uses IPA after acetone? Color is a good indication for sure.

SWIM is curious because SWIM knows for a fact that when making mescaline HCl from peyote (would be similar for any other cactus) other alkaloids are also there in the final material (SWIM made a post about an analysis that was done on such material but can't find where it is). Maybe the IPA removes them too? Because the acetone only removes the acid junk and any other really polar stuff.
 
69ron
#19 Posted : 5/27/2009 5:54:12 AM

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The odor is completely gone after cleaning with 99% IPA as well as the last bit of color the acetone can't remove. Without that, SWIM cannot get rid of the odor. The odor is strong. After the IPA wash, the oder is completely gone. Acetone just doesn't complete the job.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
burnt
#20 Posted : 5/27/2009 8:29:35 AM

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Thats interesting SWIM knows the odor SWIY is speaking of. SWIM bets its some of the other alkaloids that acetone isn't removing. Cool maybe will check out next time SWIM has material to play with.
 
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